Method of producing stearine



Patented Apr. 18, 1933 UNITED STATES PATENT OFFICE WALTEEB SCHIBAU'IH, BERLIN-DAHLEK, GERMANY METHOD 0] PIBDDUCING B'IEABINE Io Drawing. Application filed February 28, 1881, Serial No. 519,700, and in Germany February 25, 1830.

The commercial stearine, in the main a mixture of varying quantities of palmitic and stearic acid is produced even today by merely separating the fatty acid mixture 6 gained from natural animal or vegetable ats. After further treatment the olein coming from the presses is introduced in the market as such and does not always have a welcome reception in the respective induslo trial plants (as for ins nce in the textile and soap industries). method therefore that permits the manufacture of stearine without the necessit of simultaneously roducing the b -pro uct-olein, is there ore 16 a factor of the highest economical importance. I

True, experiments have been made to secure raw materials which lend themselves for the manufacture of stearine through 20 catalytical hydrogenation of vegetable or animal fats. However, the result has always beenthat the products derived after sphtting such hydrogenated fats do not come up tothe requirements of the market, since they fail to possess the properties either by their construction or by their character as such which only go to make out of a palmitic-stearic acid mixture technical stearine as we know it. Hydrated whale-oils and fish oils (glycerides) containing predominantly glycerme have proved an entirely unsatisactory starting material.

If, however, we use sperm-whale-oils (head or body oil of the bottle nose whale) also very often termed sperm-whale trane,

as a starting material, it has been found that we will then arrive at a fattyacid mixture corresponding to technical stearine. Such sperm whale oil is a hetero neous mixture of various wax-esters whic predominantly, because of their unsaturated character, are in a liquid or semiliquid state.

This oil is converted by catal 'cal h drogenation into a hard wax whic after in 'smelted with alkali and then acidified wit mineral acids yields a stearic fatty acid mixture meeting any and all technicaI requirements. a

1,000 parts by weight of sperum whale oil, for instance, with the addition of the cus- -physical and chemical values (titre etc.) are tomary technical catalyst, are subjected to the process of hydrogenation until its iodine value has scaled down practically to the zero-point and until the melting point has been raised to 50 C. The resultant hydrogenation product is separated from the catalyst and then mixed with 180-200 parts of solid caustic sodium, heating it up to 250- 280 C. in a closed autoclave. The resultant hydrogen (about 100 cubic meters) may 60 from time to time be blown off and utilized in. the hydrogenation of a new batch of sperm whale oil. The soap thus produced is reacted with dilute sulphuric acid after a preceding two hours heating process. Fre c5 quently snowy white or faintly yellow such a fatty acid mixture may then e sub ected to distillation or, if desired, to the usual refining or bleac process. The products titre amounts to a out 52 0., its iodine value ranges not much above 0.

In the place of the above mentioned caustic sodium we may, with the same success, employ caustic potassium or caustic calcium in combination with the above mentioned 76 caustic alkalies. It is known that the head or body oils of the bottle nose whale yield hard waxes with properties similar to sper maceti if subjected to catalytical hydrogenation. We also know, that higher molecular 80 aliphatic alcohols would be oxidized to the oorrespondin carbonic-acids in an alkaline smelting. e make use of this fact for instance when analyzing waxes such for example a's beeswax. But it was not known, however, that a combination of this method as applied to sperm oils, would result in products that concerning their roperties and structural character as well -as their on a par with technical stearine, thus easily taking its place.

I claim:

1. The process of manufacturing technical stearine which comprises melting substantially completely hydrogenated sperm whale oil with twice as large a quantity of sol d alkali of the group consisting of caustic soda, caustic potassium and caustic calcium as would be theoretically required to saponn fy said oil as calculated according to the saponification number and reacting the resulting soaps with mineral acids.

2. The process of manufacturing technical stearine which comprises treating substantially completely hydrogenated sperm whale oil with solid caustic alkali to produce soap and reacting the resulting product with a mineral acid.

3. The process of manufacturing technical stearine which comprises treating substantially completely hydrogenated sperm whale oil with solid caustic sodium 'at a temperature approximating 250 to 280 C. to roduce soap and reacting the resulting pro uct with mineral acid.

4. The process of manufacturing technical stearine which comprises treating substantially completely hydrogenated sperm whale oil with solid caustic alkali at a temperature approximating 250 to 280 C; to saponify the same and to oxidize the alcohol obtained in the saponification and reacting the resulting product with mineral acid.

5. The process of manufacturing technical stearine which comprises completely hydrogenating sperm whale oil, treating the hydrogenated oil with solid caustic alkali at a tem rature between 250 and 280 C. to saponify the oil and to oxidize the alcohol obtained in the saponification and reacting the resulting product with mineral acid.

6. The process of manufacturing technical stearine which comprises treating substan tially completely hydrogenated sperm whale oil with solid caustic alkali in the proportion of approximately two parts of caustic alkali to ten parts of hydrogenated oil at a temperature approximating 250 to 280 C.

to saponi the oil and to oxidize the alcohol obtained in the saponification andreacting the resulting product with mineral acl 7. The process of manufacturing technical stearine which comprises treating substantially completely hydrogenated sperm whale oil with solid caustic alkali in a proportion of approximately twice the aniount of solid caustic alkali indicated as an equivalent by the sa'ponification number of the hydrogenated oil at a temperature approximating 250 to 280 C. for approximately two hours to saponify the oil and to oxidize the alcohol obtained in the saponification and reacting the resulting product with mineral acid.

In testimony whereof I aflix my signature.

WALTHER SCHBAUTH. 

